MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 2
·1-9
·
IF 5.479
Deng Ze-Hui,Wang Xia,Wang Xiao-Li,Gao Cui-Ling,Dong Liang,Wang Ming-Lin,Zhao Ru-Song
A magnetic covalent organic framework (Fe 3 O 4 @COF) with core–shell structure was fabricated at room temperature and used as an adsorbent for magnetic solid-phase extraction of polar endocrine-disrupting phenols (4-n-nonylphenol, 4-n-octylphenol, bisphenol A and bisphenol AF). The sorbent was characterized by transmission electron microscopy, FTIR, powder X-ray diffraction and other techniques. The main parameters governing the extraction efficiency were optimized. The phenols were quantified by HPLC with fluorometric detection. The method has attractive features such as low limits of detection (0.08–0.21 ng.mL −1 ), wide linear ranges (0.5–1000 ng.mL −1 ), and good repeatability (intra-day: 0.39%–4.99%; inter-day: 1.57%–5.21%). Satisfactory results were obtained when the developed method was applied to determine the four target pollutants in real world drink samples with spiked recoveries over the range of 81.3~118.0%. This indicates that the method is a powerful tool for the enrichment and determination of endocrine-disrupting phenols in drink samples.
A magnetite based covalent organic framework (Fe 3 O 4 @COFs) was synthesized with TPAB, TPA and Fe 3 O 4 . It was used for magnetic solid-phase extraction of endocrine-disrupting phenols from plastic-packaged tea drink samples coupled with liquid chromatography (LC) for determination.
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高影响因子
MOLECULES
·
2019
·Vol. 24
·期 7
·1439
·
IF 3.06
Ling Li Chen,Shan Shan Chu,Ling Zhang,Jin Xie,Min Dai,Xin Wu,Hua Sheng Peng
Background: Qianhu is a traditional Chinese medicine. It is thought that Qianhu roots will harden after bolting and not be suitable for medicinal purposes. Bolting Qianhu and unbolting Qianhu are referred to as “Xiong Qianhu” and “Ci Qianhu,” respectively. In this study, the properties, microscopic and chemical characteristics of Ci Qianhu and Xiong Qianhu roots were compared using fluorescence microscopy, laser microdissection coupled with ultra-high-performance liquid chromatography-quadrupole/time-of-flight mass spectrometry, and high-performance liquid chromatography with diode-array detection. Results: Microscopy results showed that the area of secondary xylem in the root increased after bolting, with the cork and secretory canals showing strong fluorescence intensity. A total of 34 peaks, mostly pyranocoumarins, were identified in the tissues of Ci Qianhu and Xiong Qianhu. The secretory canals contained the highest variability of coumarins, whereas the secondary xylem contained the least coumarins. Moreover, seven coumarins, especially the pyran- coumarin, decreased after bolting. Generally, both before and after bolting, coumarin level was the highest in the bark, followed by the middle part, and the lowest in the inner part. Conclusion: Thus, it was indicated that the area of secondary xylem increased after bolting, however the coumarin variant and content decreased in the secondary xylem of Qianhu. The result shows that the quality of Qianhu decreases after bolting, which supports the viewpoint that Xiong Qianhu is not suitable for medicinal use.Keywords:bolting;Peucedanum praeruptorumDunn;microstructure;LMD;UPLC-Q/TOF–MS;HPLC–DAD
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 2
·1-8
·
IF 5.479
Xia Hongjun,Wang Jun,Chen Gang,Liu Jiawei,Wan Guangpin,Bai Quan
Monodisperse SiO 2 @SiO 2 core-shell silica microspheres (CSSM) with enlarged mesopores perpendicular to the particles surface were prepared using a dual-templating approach. With cetyltrimethyl ammonium bromide as the template and octyltrimethyl ammonium bromide as an auxiliary chemical, the pore size can be enlarged from 2.6 to 10.6 nm. The average shell thickness can be increased from 31 nm to 97 nm by adjusting the concentrations of the surfactants under continuous addition of tetraethyl orthosilicate. After coating twice, the resulting CSSM has a uniform mesoporous shell of about 198 nm thickness and a narrow pore size distribution. The CSSM were then modified with octadecyltrichlorosilane to give a material referred to as CS-C18. It was evaluated by separating the mixture of methylbenzene (toluene), ethylbenzene, n-propylbenzene, n-butylbenzene, n-amylbenzene and hexylbenzene. The baseline separation of the six alkyl benzenes is achieved within 2 min. Compared to a commercial column of type BEH-C18, CS-C18 shows a faster and better separation even at lower back pressure. It was also applied to the fast separation of benzo[a]pyrene, salbutamol, ractopamine and clenbuterolin residues in pork samples. The high column efficiency and better reproducibility suggest that the CSSM can be used as a matrix for fast separation and analysis of several kinds of small analytes.
A dual-templating approach was utilized to produce the core shell microsphere with controllable mesopore channels by using hexadecyltrimethylammonium bromide (CTAB) as the template and trioctylmethylammonium bromide (TOMAB) as an auxiliary chemical to enlarge the size of CTAB micelles.
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Analytical Methods
·
2016
·Vol. 8
·期 6
·1405-1414
·
IF 1.915
Na Cao,Lei Liu,Yuan-bin Hao,Li-li Sun,Qiao-gen Zou,Xing-ling Ma,Kai-he Xiong
A sensitive, rapid and stable HPLC-MS/MS method has been developed and validated for the determination of rabeprazole enantiomers and their four metabolites, namely rabeprazole thioether, rabeprazole sulfone and desmethyl rabeprazole enantiomers, in beagle dog plasma using esomeprazole as the internal standard. The analytes and the internal standard were extracted from plasma samples by liquid–liquid extraction and separated on a Chiral-HSA column using acetonitrile-10 mmol L−1 ammonium acetate as the mobile phase by gradient elution. The method was validated with respect to sensitivity, specificity, linearity, precision, accuracy and especially the stability of analytes under various conditions, and was successfully applied in evaluating the pharmacokinetic profiles of racemic rabeprazole, the pure enantiomers and their metabolites in beagle dogs after single intravenous administration of (R)-rabeprazole sodium injection (at 0.33, 1 and 3 mg kg−1), (S)-rabeprazole sodium injection (at 1 mg kg−1) and racemic rabeprazole sodium injection (at 2 mg kg−1). The two enantiomers showed different profiles of pharmacokinetic parameters. The AUC0–t and t1/2 values of (R)-rabeprazole were higher and the clearance (CL) value of (R)-rabeprazole was lower than that of (S)-rabeprazole. Compared to (S)-rabeprazole, the higher absorption and slower elimination of (R)-rabeprazole explain why (R)-rabeprazole is more effective than the racemate.
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Analytical Methods
·
2017
·Vol. 9
·期 18
·2673-2681
·
IF 1.9
Lingling Wang,Qi Li,Lei Zhang
An elastic cylindrical three-dimensional porous spongy graphene rod (3D-PSGR) was synthesized by a facile one-step hydrothermal method and applied in a syringe system as a solid phase adsorbent for the extraction of nine trace bisphenol analogs (BPs) from environmental samples. In this study, a simple sample pretreatment procedure in-syringe-assisted solid phase microextraction (ISA-SPME) was developed for the detection of nine BPs with HPLC. The full protocols for the extraction and elution process were achieved in a syringe. After enrichment, the sample solution was expelled slowly from the syringe to leave the adsorbent with the analytes behind. The analyte-enriched adsorbent was then eluted by drawing MeOH into the syringe, and the elution solution was then injected in HPLC. The 3D-PSGR exhibits excellent cycling stability and can be reused for eight consecutive cycles without significant loss of extraction efficiencies. The 3D-PSGR-ISA-SPME was applied successfully to the analysis of nine BPs in river water and soil samples. The method detection limits (MDLs) were in the range of 0.39–3.97 ng mL−1, and the extraction recoveries of the spiked samples were in the range of 96.5–102.6% with relative standard deviations (RSDs) of 2.11–4.27%. A convenient method is proposed for the analysis of nine trace BPs in environmental samples.
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CHROMATOGRAPHIA
·
2024
·Vol. 87
·期 6
·407-418
·
IF 1.2
Hong Lei,Mao Huihui,Huang Xiaowei,Fu Xinyang,Lin Yanfang
To analyze 1-methyladenosine (m1A) and 1-methylinosine (m1I) in urine samples obtained from patients with breast cancer and healthy people, we used magnetic dispersive solid-phase micro-extraction (MDSPME) combined with high-performance liquid chromatography. The structure and morphology of magnetic nanoparticles, Fe 3 O 4 @GO, were investigated by FT-IR, XRD, TEM, and TGA. m1A and m1I in urine samples were enriched by the solid phase micro-extraction technology of Fe 3 O 4 @GO. Several parameters affecting the extraction efficiency, including adsorption time, pH, ionic strength, mass of adsorbent, extraction time, eluent solvent, elution time, and elution temperature, were researched and optimized. Under the optimized conditions, the corresponding linearity range of the two analytes showed a good linearity ( r 2 > 0.9998) and significant addition recoveries ranging from 88.50 to 109.38%, while the limit of detection was between 0.10 and 0.11 ng/mL. The enrichment factors of m1A and m1I were 108 and 134, respectively. The method was simple, sensitive, and reliable for the detection and purification with good detection limit, and it was suitable for the detection of m1A and m1I in urine samples. In addition, the analysis of modified nucleosides is of great value for the early diagnosis of patients with breast cancer.
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ANALYTICA CHIMICA ACTA
·
2025
·
IF 6
Xiaoqian Yuan,Yuchen Cui,Yaqin Nan,Ruijun Tang,Xinru Wang,Yanmei Xu,Xinghua Jin,Yiwen Wang,Ding Cheng,Youxin Li
Background Cyclodextrins (CDs) and their derivatives have been widely used as chiral selectors in HPLC. However, many derivatized CDs lack specificity for certain drugs and often exhibit limited resolution. Furthermore, their synthesis typically involves complex multi-step procedures, hindering scalability and cost-efficiency. To overcome these limitations, this study aims to develop a simple and scalable boric acid-modified β-cyclodextrin polymer (BA-β-CDP), targeting chiral substances with O/N atoms in chiral and/or adjacent carbons. Results BA-β-CDP was synthesized on a large scale using inexpensive reagents and a random substitution strategy, avoiding tedious protection-purification steps. Structural and chromatographic compatibility was confirmed by nine characterization techniques. In HPLC using the chiral mobile-phase additive (CMPA) method, BA-β-CDP enabled the efficient separation of 25 racemates. Among them, 24 achieved complete or baseline separation, and 10 exhibited resolution (Rs) values > 10. Typical cases included bisoprolol (Rs = 48.19), propranolol (Rs = 45.50), chlorpheniramine (Rs = 38.36), and metoprolol (Rs = 20.26). Additionally, the material demonstrated excellent batch-to-batch reproducibility, recyclability, and reusability. Significance and novelty This work presents a practical and cost-effective chiral selector. The synergistic mechanism offers strong and specific recognition toward chiral substances with O/N atoms in chiral and/or adjacent carbons. This approach represents a novel strategy for efficient and economical HPLC-based enantioseparation using widely accessible materials and methods.
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FOOD CHEMISTRY
·
2021
·
IF 7.514
Kaige Zhang,Yunhe Wang,Shuangying Li,Guifen Zhu
Deep eutectic solvents (DESs) are a new class of green “designer solvent”; its physicochemical properties can be easily tuned by adjusting DES′ constituents, chemical ratio and water content. In this study, three hydrophobic DESs with low viscosity, low density, and melting points close to room temperature were designed and synthesized. Based on these DESs , an air-assisted liquid–liquid microextraction technique was developed based on the solidification of floating DESs for the simultaneous determination of bisphenols and polycyclic aromatic hydrocarbons (PAHs) via HPLC. The microextraction parameters were optimized via the Plackett-Burman design and response surface methodologies. The method shows satisfactory linearity (R 2 ≥ 0.9928), a low limit of detection (0.16–0.75 μg L −1 ) and satisfactory precision (≤2.3%), and was successfully applied for the simultaneous determination of bisphenols and PAHs from tea infusions with satisfactory recoveries (82.0–116.6%). This method is simple, rapid, economical, environmentally compatible, dispersive solvent-frees and centrifugation-free, and has promising applications in food safety.
研究领域:
分析化学
·
食品安全
·
环境科学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2026
·
IF 2.5
Yuxing Liu,Yan Yan,Changjian Wu,Kangwei Shen,Wei Fan,Mengjie Li,Hai Zhao,Yi Cao,Xuejun Kang,Penglin Wu,Dianzhi Liu
PAN/PPy NFs are first applied to PFSPE-HPLC-FLD for urinary pteridines detection. • PAN/PPy NFs adsorb pteridines via synergistic electrostatic, H-bond and π-π forces. • The optimized method gives negligible matrix effects (−6.6%–8.2%) for urine samples. • The sensitive, robust method was fully validated for clinical urine sample analysis. Pteridines are associated with neuroinflammation and oxidative stress, the core pathological processes of autism spectrum disorder (ASD). Urinary neopterin (NPT), biopterin (BPT), and isoxanthopterin (IXP) are promising non-invasive biomarkers for children with ASD. However, matrix interference from urinary salts and metabolites severely impedes trace pteridine detection, while mainstream analytical methods either require cumbersome derivatization or sacrifice sensitivity for dilution to mitigate matrix effects (ME). This study reports the first application of polyacrylonitrile/polypyrrole nanofibers (PAN/PPy NFs) for the determination of pteridines in urine by packed-fiber solid-phase extraction (PFSPE) coupled with HPLC-FLD, without derivatization. XPS, FTIR and fluorescence experiments confirmed pteridine adsorption on PAN/PPy NFs via synergistic electrostatic attraction, hydrogen bonding and π-π stacking. Validation showed: ME -6.6%–8.2%, R 2 > 0.995, LOD s 0.8–5.3 ng/mL, LOQ s 2.8–17.6 ng/mL, and RSD s < 9.7%. AGREE (0.61) and BAGI (72.5) verified its compliance with green analytical chemistry principles. Analysis of 33 ASD and 34 healthy urine samples revealed significantly elevated NPT levels in the ASD group ( p = 0.011). This efficient, sensitive and green PFSPE-HPLC-FLD method eliminates urinary matrix interference without derivatization, overcoming key limitations of conventional approaches. It provides a reliable tool for urinary pteridine assays in ASD research and supports ASD pathogenesis investigation and exploratory clinical studies. The figure shows PAN/PPy-PFSPE for matrix effect elimination from ASD children's urine. PAN/PPy NFs sorbent, with high porosity and multiple interaction sites, mediates pteridine adsorption via synergistic electrostatic attraction, hydrogen bonding and π-π stacking, enabling rapid green purification and ultrasensitive simultaneous detection of urinary NPT, IXP and BPT for exploratory clinical studies. Download: Download high-res image (154KB) Download: Download full-size image
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FOOD CHEMISTRY
·
2021
·
IF 7.514
Guohao Cheng,Juan Zhao,Xiaoyue Wang,Can Yang,Shiying Li,Tong Lu,Xiang Li,Xuefeng Wang,Guifen Zhu
The effective analysis of cephalosporin antibiotics in food animals has attracted considerable attention. Herein, a high-performance liquid chromatograph equipped with a UV method based on molecularly imprinted-solid phase extraction (MISPE-HPLC-UV) was developed for preconcentration, cleanup and determination of ceftiofur sodium (CTFS) in food samples. In this method, an eco-friendly molecularly imprinted polymer (MIP) was synthesized and employed as an adsorbent, which exhibited excellent selectivity towards CTFS in water, and adsorption equilibrium could be reached within 1 h. Under the optimized conditions, good linearity was obtained for CTFS in the range of 0.005–1.0 mg L −1 with a lower LOD of 0.0015 mg L −1 , and the average recoveries were higher than 91.9% (RSD less than 8.5%) at three spiked levels in milk, chicken, pork and beef samples. After 20 cycles, the recovery of the MISPE cartridge for CTFS was still higher than 95%, which proved that the MISPE-HPLC-UV method was highly sensitive and selective for the analysis of CTFS in food samples.
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MICROCHIMICA ACTA
·
2020
·Vol. 187
·期 1
·1-9
·
IF 6.232
Chen Jianxiong,Zhang Birong,Dang Xueping,Zheng Dongyun,Ai Youhong,Chen Huaixia
A polyaniline composite doped with etched multi-walled carbon nanotubes and UiO-66-NH 2 was prepared by electropolymerization. It was used as a sorbent to extract the polycyclic aromatic hydrocarbons (PAHs) phenanthrene, fluoranthene and pyrene. Its surface morphology, crystal structure and capability of adsorbing PAHs were characterized by scanning electron microscopy, X-ray photoelectron spectrometry, Fourier transform infrared spectrometry and zeta potentiometry. The π stacking and anion-π interactions are shown to play dominant roles in the sorption mechanism. Coupled with high performance liquid chromatography, the composite-modified fiber was applied to detect PAHs in lake water samples by direct immersion extraction. The method excels by (a) wide linear range (0.05–20 ng mL −1 ), (b) low limits of detection (10 pg mL −1 ), (c) satisfactory recovery from spiked samples (84.7–113.8%), and (d) good reproducibility (relative standard deviations of <6.5%). The method is superior in terms of costs and reproducibility compared to some pretreatment methods with mass spectrometric detection.
Schematic representation for interaction between PANI-etched MWCNT/UiO-66-NH 2 and polycyclic aromatic hydrocarbons (phenanthrene, fluoranthene, pyrene).
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Food Chemistry-X
·
2023
·
IF 6.1
Yiwei Tang,He Meng,Wenxiu Wang,Yang Song,Shuo Wang,Zhuanying Li,Xianghong Wang,Xuelian Hu
An innovative core–shell magnetic molecularly imprinted polymers, Fe 3 O 4 @SiO 2 @MIPs, was elaborately tailored for specific separation and enrichment of olaquindox (OLA) and its metabolic marker methyl-3-quinoxaline-2carboxylic acid (MQCA). Herein, benefiting from the combination of functionalized magnetic nanoparticles (Fe 3 O 4 @SiO 2 ) and MIPs, Fe 3 O 4 @SiO 2 @MIPs not only possessed favorable magnetic properties and stability, avoiding tedious sample pretreatment process, but also demonstrated exceptional selective recognition ability and adsorption capacity, suppressing influence of coexisting interfering substances. Encouraged by prominent merits, Fe 3 O 4 @SiO 2 @MIPs-based magnetic solid phase extraction with HPLC method was developed, realizing simultaneous measurement of OLA and MQCA. Under optimal conditions, excellent linear ranges of 0–100 μg/L with detection limit of 0.175–0.271 μg/L were obtained. The proposed method was finally utilized for determination of OLA and MQCA in fish muscle and milk samples with satisfactory recoveries (80.56–95.26%) and relative standard deviation below 8.1%, furnishing a reliable and sensitive strategy for enrichment and detection residual veterinary drugs in food samples.
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